Laboratory Methods of Inorganic Chemistry, 2nd English Ed. 1928

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114 OXY-HALOGEN ACIDS.


of the powder thus obtained with 75 g. of potassium dichromate


which has been dried by being melted. Heat the mixture in the


iron dish already used, whereupon the reaction will begin in spots


and spread with incandescence throughout the mass. Pulverize
the loose black product while still warm, cover it in a flask with a


warm mixture of 450 c.c. 80% ethyl alcohol and 50 c.c. of methyl


alcohol and boil it with a return condenser on the water bath for


two minutes. Decant the hot solution through a plaited filter into
a beaker, which is cooled with ice, and allow the salt to crystallize


while stirring. Using the mother-liquor from this crystallization


as a solvent, extract the black mass again in the same manner as


before; filter, and repeat the extraction three or four times.
Collect all of the cyanate crystals on the same suction filter, and


after washing with ether, dry them in a vacuum desiccator over


sulphuric acid. Yield, 30-40 grams. The product may be used


in the preparation of urea, or of semicarbazid, No. 123.


Urea from Ammonium Cyanate.
Ammonium cyanate when heated in aqueous solution undergoes a trans-
formation into urea (Wohler, 1828).


NH 4 CNO = CO(NH 2 ) 2.

To carry out this classic reaction, evaporate a solution of 8.1 g.


potassium cyanate and 8.0 g. ammonium nitrate to dryness on the


water bath. Boil the powdered residue in a flask twice with alco-
hol, and concentrate the extract until a crystallization in fine, long


needles is obtained. Yield, about 5 g.


Heat a pinch of dry urea in a test-tube until it just melts, and


keep it at this temperature for about a minute; ammonia escapes.


Dissolve the residue in a little water and add a drop of copper sul-
phate solution and some sodium hydroxide, whereupon a rose-


violet coloration appears; this is the so-called biuret reaction.


(6) Oxy-halogen Acids.



  1. Electrolytic Production of Sodium Hypochlorite and Potassium


Chlorate.
Sodium hydroxide and chlorine react in cold, aqueous solution, forming
sodium hypochlorite, sodium chloride and water.
2 NaOH + Cl 2 = NaCl + NaCIO + H 2 O.


As soon as chlorine is present in excess, it reacts to produce free hypochlo-
rous acid,
HOH + Cls = HOC1 + HC1;

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